3-Phenylprop-2-Enal → alpha-Bromocinnamaldehyde

HRID 555974

反応式

HRID 555974 の反応式
[CH:1](=[O:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br:11]Br.C([O-])([O-])=O.[K+].[K+].O>C(O)(=O)C>[Br:11][C:2](=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH:1]=[O:10]

参加物

6

反応物 4

HCID 3073-Phenylprop-2-EnalHCID 962WaterHCID 11430Potassium CarbonateHCID 24408Bromine

生成物 1

HCID 21585alpha-Bromocinnamaldehyde

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1.33 g (10 mmol) cinnamaldehyde was dissolved in 5 mL glacial acetic acid and cooled on an ice-water bath. 1.62 g bromine was added, and anhydrous K2CO3 was then added, and it was stirred until no gas was evolving. After refluxing for 30 min, the reaction mixture was poured into 100 mL cold water with stirring, extracted with 50 mL ethyl ether three times. The combined ethyl ether layers were washed with water one time, saturated aqueous NaCl solution one time, dried over MgSO4 for 2 hours, filtrated, and the filtrate was dried under vacuum, and washed with anhydrous ethyl ether: petroleum ether (1:1) to give the title compound as light yellow powder.

後処理

  1. temperaturecooled on an ice-water bath
  2. temperatureAfter refluxing for 30 min
  3. stirringwith stirring
  4. extractionextracted with 50 mL ethyl ether three times
  5. washThe combined ethyl ether layers were washed with water one time, saturated aqueous NaCl solution one time
  6. dry with materialdried over MgSO4 for 2 hours
  7. filtrationfiltrated
  8. customthe filtrate was dried under vacuum
  9. washwashed with anhydrous ethyl ether: petroleum ether (1:1)

出典と根拠

ORDレコード
ord-33127781f18340369da56dfe4b8793c5
出典データセット
uspto-grants-2011_11
特許番号
US08053577B2

関連ノート

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